CN102585602A - Noble metal replacing catalysis ink for printing circuit - Google Patents
Noble metal replacing catalysis ink for printing circuit Download PDFInfo
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- CN102585602A CN102585602A CN201210031150XA CN201210031150A CN102585602A CN 102585602 A CN102585602 A CN 102585602A CN 201210031150X A CN201210031150X A CN 201210031150XA CN 201210031150 A CN201210031150 A CN 201210031150A CN 102585602 A CN102585602 A CN 102585602A
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Abstract
The invention relates to a noble metal replacing catalysis ink for a printing circuit. The noble metal replacing catalysis ink is characterized by mainly consisting of 10 to 90 percent of functional materials, 2 to 18 percent of organic carriers and 8 to 72 percent of organic solvents, wherein the functional materials consist of metal or/and metal oxide powder, the metal is selected from on kind of metals of iron, nickel, aluminum and zinc or is a mixture formed by at least two kinds of metals in five metals of iron, nickel, aluminum, zinc and copper according to any weight proportions, and the metal oxide is selected from ferrous oxide or/and cuprous oxide. The noble metal replacing catalysis ink can be manufactured on an insulation substrate by adopting the traditional printing modes of screen printing, intaglio printing and the like, and then, the noble metal replacing catalysis ink can be placed into replacement reaction solution for taking replacement reaction for forming a conductor printing circuit. The noble metal replacing catalysis ink has the characteristics that: 1, the ink does not contain noble metals of sliver, gold and the like, so the manufacture cost of relevant products is greatly reduced; 2, the use method is simple; and 3, the manufactured printed circuit is reliable, the conducting performance is good, and the application is wide.
Description
Technical field
The present invention relates to make the novel ink of used for printed circuit, particularly a kind of used for printed circuit catalytic ink that can replace precious metal.This catalytic ink has replaced precious metal printing ink such as traditional argentiferous, gold, platinum, palladium, can be through traditional printing mode such as silk screen printing, intaglio and use spraying, the mode of whitewashing makes various printed wiring cheaply on the exhausted base material of edge.
Background technology
At present, printed wiring is widely applied in products such as thin film switch, electronic tag, touch-screen, PC board, flexible PCB or component.Usually the making method of printed wiring is to be printed onto electrically conductive ink (or claiming electrocondution slurry) on the exhausted base material of edge through traditional printing modes such as silk screen printing, intaglios; And then through in, low temperature is cured, thereby on the exhausted base material of edge, formed printed wiring.But all contain noble metal powders such as silver, gold, platinum, palladium in the electrically conductive ink of above-mentioned use, thereby cause this electrically conductive ink to cost an arm and a leg, improved the cost of finished product greatly.And replace precious metals such as silver, gold with copper base metal, nickel, because oxidation easily can form oxide skin on its surface in the course of processing, thereby cause non-conductive.And carbon can not satisfy the requirement of low-resistivity circuit because electric conductivity is low.So this be at present in all, low-temperature cured conductive printing ink all contains the true cause of noble metal powder such as silver powder.Such as U.S. Advanced Products, the electrically conductive ink that Inc company produces adds the silver powder of 50～70% weight in organic carrier, and the electrically conductive ink of processing is used for making thin film switch (seeing U.S. Pat 5200264); The J.R.Dorfman of du pont company is well-dispersed in silver powder in the carrier that contains chlorine vinegar resin, produces the antenna (see U.S. Pat 7857998B2) of the circuit of low-resistivity with electronic tag.But expensive silver powder has all inevitably been used in these inventions, causes its product cost to increase greatly thus.Therefore how developing the electrically conductive ink that is made up of base metal is the problem that those skilled in the art study.
Summary of the invention
The present invention provides a kind of used for printed circuit catalytic ink that replaces precious metal, its objective is and will develop a kind of electrically conductive ink that is made up of base metal, to reduce the manufacturing cost of related prods.
For achieving the above object, the technical scheme that the present invention adopts is: a kind of used for printed circuit catalytic ink that replaces precious metal, and this catalytic ink comprises following component and weight percentage thereof:
(1) functional materials 10～90%
Said functional materials is by metal, perhaps MOX, and perhaps metal and MOX mix by any part by weight and constitute, and the particle diameter of functional materials is at 30 nanometers～25 micrometer ranges;
Said metal is selected one of iron, nickel, aluminium, four kinds of metals of zinc, perhaps in iron, nickel, aluminium, zinc, five kinds of metals of copper at least two kinds of metals by the mixture of any part by weight;
Ferrous or the Red copper oxide of said MOX selective oxidation, perhaps iron protoxide and Red copper oxide are by the mixture of any part by weight;
(2) organic carrier 2～18%
Said organic carrier is by constituting in the following high molecular polymer a kind of or two or more the mixing by any part by weight:
Urethane;
Polycarbonate;
SE;
Polymethylmethacrylate;
Phenoxy resin;
Polyester;
Ethylene copolymer;
In the above organic carrier, said polyester is polyethyleneterephthalate, polybutylene terephthalate, poly terephthalic acid diallyl, ekonol, unsaturated polyester resin, resol or vinyl resin;
In the above organic carrier; The polymkeric substance that said ethylene copolymer is formed by two or more monomer copolymerization that contains vinyl, the said monomer that contains vinyl has: vinyl acetate, vinyl alcohol, vinylchlorid, vinylidene chloride, vinylbenzene, vinyl cyanide, hydroxyalkyl acrylates, TEB 3K, methyl acrylate, ethyl propenoate, n-butyl acrylate and 2 ethyl hexyl acrylate;
(3) organic solvent 8～72%
Said organic solvent is selected a kind of solvent in following ether solvent, esters solvent, ketones solvent and the alcoholic solvent, and perhaps two or more solvents are pressed the mixture of any part by weight:
Ether solvent has:
Diethylene glycol ether;
Propylene glycol monomethyl ether;
Dipropylene glycol methyl ether;
The dipropylene glycol propyl ether;
Propylene glycol propyl ether;
The Ucar 35 butyl ether;
The dipropylene glycol butyl ether;
The tripropylene glycol butyl ether;
The Ucar 35 phenylate;
The dipropylene glycol dme;
Esters solvent has:
ETHYLE ACETATE;
The diethylene glycol monobutyl ether acetic ester;
1-Methoxy-2-propyl acetate;
Dipropylene glycol methyl ether acetate;
PGDA;
The amyl acetate-n mixture;
N-butyl acetate;
Isobutyl acetate;
N-propyl acetate;
Iso Butyl Acetate;
N-butyl propionate;
The 3-ethoxyl ethyl propionate;
Witcizer 300;
The propionic acid n-pentyl ester;
The propionic acid n-propyl;
Dibasic acid esters;
Ketones solvent has:
Acetone;
Butanone;
Alcoholic solvent has:
α-or β-Terpineol 350;
Diethylene glycol monobutyl ether;
Pinakon;
Amyl alcohol mixture;
Propyl carbinol;
Isopropylcarbinol;
Virahol;
Diisobutyl carbinol(DIBC);
Methyl isobutyl carbinol;
The 2-methyl butanol;
Pentyl alcohol;
N-propyl alcohol;
Exxal 12.
Related content in the technique scheme is explained as follows:
1. in the such scheme, said " printed wiring " be meant adopt printing ink and through traditional printing mode such as silk screen printing, intaglio and use spraying, various conducting channels that the mode of whitewashing is made on the exhausted base material of edge.
2. in the such scheme, the preferable content range of each component is: the content of said functional materials is 40～80%; The content of said organic carrier is 3～15%; The content of said organic solvent is 16～48%.The best content range of each component is: the content of said functional materials is 50～75%; The content of said organic carrier is 5～10%; The content of said organic solvent is 20～40%.
3. in the such scheme, functional materials, organic carrier and organic solvent are that catalytic ink of the present invention is realized the requisite key component of its purpose, with the exception of this, can also add some auxiliary agents in order further to improve effect.Said assistant packet contains dispersion agent 0.2～1.5%; Reductive agent 1～5%; Thixotropic agent 0.2～2%; Flow agent 0.2～2% or the like.Wherein, The effect of dispersion agent is that the help function dispersion of materials is even; That dispersion agent adopts is cationic, a kind of in anionic, non-ionic type and the amphoteric, and wherein, cationic have polymine, the two ammonio methacrylates of two octadecyl or an imidazoline quaternary ammonium salt; Anionic is a soybean lecithin; Non-ionic type is an AEO; Amphoteric is the cocoyl azochlorosulfonate propyl lycine.Reductive agent adopts at least a in glucose, formaldehyde, inferior sodium phosphate, boranes material and the Hydrazine Hydrate 80.Thixotropic agent adopts nano-carbon powder, nano silicon or organobentonite.
Principle of work of the present invention is: catalytic ink of the present invention is different fully with the principle that existing electrically conductive ink forms printed wiring.Existing electrically conductive ink itself has electroconductibility, needs only during use through traditional printing modes such as silk screen printing, intaglios to be printed onto on the exhausted base material of edge, and then directly on the exhausted base material of edge, forms printed wiring through being heating and curing.And catalytic ink of the present invention itself does not have electroconductibility, electricalresistivity＞2 * 10
8Ω cm; To or use the mode that sprays, whitewashes on the exhausted base material of edge, to make ink traces during use earlier through traditional printing modes such as silk screen printing, intaglios; Make ink traces dry then through heating; To put into replacement(metathesis)reaction solution with the exhausted base material of the edge of ink traces at last and carry out electroless plating, thereby form the conductor printing circuit.So-called electroless plating is actually the metal that makes in the printing ink or MOX and replacement(metathesis)reaction solution metal ion and carries out replacement(metathesis)reaction, and atoms metal closely is attached to the ink traces surface, thereby on the ink traces basis, forms conductor circuit.Its mechanism of action is: metal or the MOX low with redox potential come high metal of reduction-oxidation reduction potential or MOX.Such as, containing iron in the catalytic ink, replacement(metathesis)reaction solution can adopt copper sulfate, and its replacement(metathesis)reaction formula is: Fe (catalytic ink)+Cu
2+(copper sulfate) → Fe
2+/3+(reaction back solution)+Cu (separating out copper)
The relation of metal that contains in the catalytic ink in the present invention, or MOX and spendable replacement(metathesis)reaction solution kind such as following table 1:
Table 1:
| Catalytic ink | Copper sulfate | Cupric chloride | Ferric sulfate | Single nickel salt |
| Iron | Available | Available | ||
| Nickel | Available | Available | ||
| Aluminium | Available | Available | Available | Available |
| Zinc | Available | Available | Available | Available |
| Iron protoxide | Available | Available | Available | Available |
| Red copper oxide | Available | Available |
Because the technique scheme utilization, the present invention compared with prior art has advantage and effect:
1. do not contain precious metals such as silver, gold, platinum, palladium in the catalytic ink of the present invention, and easy acquisition of employed replacement(metathesis)reaction solution and low price, so greatly reduce the manufacturing cost of related prods.
2. the method for use of catalytic ink of the present invention is simple, and is easy and simple to handle, realizes easily.
3. reliable by the printed wiring of catalytic ink making of the present invention, resistivity is low, conduct electricity very well, and be 5.5 ohm (the sample figure is: 1 meter of line length, 0.4 millimeter of live width) through measure sample resistance.
4. catalytic ink applied range of the present invention is suitable for making the various printed wiring in products such as thin film switch, electronic tag, touch-screen, PC board, flexible PCB or the component.
Embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment: a kind of used for printed circuit catalytic ink that replaces precious metal
This catalytic ink is mixed by a certain percentage by each starting material and forms.
Table 2: be formula for raw stock (the material numerical value unit: weight %) of embodiment 1～10
The preparation method of embodiment 1～10: according to the formula for raw stock in the table 2, be dissolved in organic carrier in the organic solvent earlier, add functional materials and auxiliary agent then, fully dispersed with stirring is even, promptly obtains catalytic ink of the present invention.
Using method for printing screen on the PET film, to print wide during use is 0.4 millimeter; Length is 1 meter circuit, puts into 150 degree oven dryings again 60 minutes, and then carry out electroless plating: putting into concentration to dried sample is 0.65M; The pH value is in 3 the copper-bath 2 minutes; Take out sample, drying is 20 minutes in 100 degree baking ovens, and the measure sample resistance value is seen table 2.
Electroplate: the sample after electroless plating, putting into concentration is 0.65M, and pH value is that logical 0.25 ampere electric current was electroplated 45 minutes in the electrolytic plating pool of 3 copper-bath, and the taking-up sample was spent in the baking ovens drying 20 minutes 100, and the measure sample resistance value is seen table 2.
Table 3: be formula for raw stock (the material numerical value unit: weight %) of embodiment 11～20
The preparation method of embodiment 11～20 is identical with embodiment 1～10 in the table 3, no longer is repeated in this description here.
Table 4: be formula for raw stock (the material numerical value unit: weight %) of embodiment 21～30
The preparation method of embodiment 21～30 is identical with embodiment 1～10 in the table 4, no longer is repeated in this description here.
The related problems of the embodiment of the invention are explained as follows:
1. among 30 embodiment of table 2 of the present invention～table 4, what organic carrier adopted respectively is urethane, polyester, vinyl chloride-vinyl acetate copolymer, vinyl resin, resol, vinyl acetate between to for plastic-vinyl chloride-ethylene alcohol copolymer, phenoxy ester and vinyl acetate between to for plastic-vinylchlorid-hydroxyalkyl acrylates multipolymer.With the exception of this, organic carrier can also adopt polycarbonate, SE, polymethylmethacrylate and the mutual combination between them or the like all can embodiment of the present invention, and obtains technique effect identical or that be equal to.
2. among 30 embodiment of table 2 of the present invention～table 4, what organic solvent adopted respectively is ETHYLE ACETATE, butanone, dipropylene glycol methyl ether ester acid esters, diethylene glycol monobutyl ether acetic ester, diethylene glycol ether, propylene glycol monomethyl ether ester acid esters, ethanol, α Terpineol 350 and diethylene glycol monobutyl ether.With the exception of this; Organic solvent can also adopt propylene glycol monomethyl ether, dipropylene glycol methyl ether, dipropylene glycol propyl ether, propylene glycol propyl ether, Ucar 35 butyl ether, dipropylene glycol butyl ether, tripropylene glycol butyl ether, Ucar 35 phenylate, dipropylene glycol dme, PGDA, amyl acetate-n mixture, n-butyl acetate, isobutyl acetate, n-propyl acetate, Iso Butyl Acetate, n-butyl propionate, 3-ethoxyl ethyl propionate, Witcizer 300, propionic acid n-pentyl ester, propionic acid n-propyl, dibasic acid esters, acetone, β-Terpineol 350, pinakon, amyl alcohol mixture, propyl carbinol, isopropylcarbinol, Virahol, diisobutyl carbinol(DIBC), methyl isobutyl carbinol, 2-methyl butanol, Pentyl alcohol, n-propyl alcohol, Exxal 12 and the mutual combination between them or the like all can embodiment of the present invention, and obtains technique effect identical or that be equal to.
3. among 30 embodiment of table 2 of the present invention～table 4, that dispersion agent adopts is cationic, a kind of in anionic, non-ionic type and the amphoteric, and wherein, cationic have polymine, the two ammonio methacrylates of two octadecyl or an imidazoline quaternary ammonium salt; Anionic is a soybean lecithin; Non-ionic type is an AEO; Amphoteric is the cocoyl azochlorosulfonate propyl lycine.Reductive agent adopts at least a in glucose, formaldehyde, inferior sodium phosphate, boranes material and the Hydrazine Hydrate 80.Thixotropic agent adopts nano-carbon powder, nano silicon or organobentonite.
The foregoing description only is explanation technical conceive of the present invention and characteristics, and its purpose is to let the personage who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalences that spirit is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (6)
1. used for printed circuit catalytic ink that replaces precious metal, it is characterized in that: this catalytic ink comprises following component and weight percentage thereof:
(1) functional materials 10 ~ 90%
Said functional materials is by metal, perhaps MOX, and perhaps metal and MOX mix by any part by weight and constitute, and the particle diameter of functional materials is at 30 nanometers ~ 25 micrometer ranges;
Said metal is selected one of iron, nickel, aluminium, four kinds of metals of zinc, perhaps in iron, nickel, aluminium, zinc, five kinds of metals of copper at least two kinds of metals by the mixture of any part by weight;
Ferrous or the Red copper oxide of said MOX selective oxidation, perhaps iron protoxide and Red copper oxide are by the mixture of any part by weight;
(2) organic carrier 2 ~ 18%
Said organic carrier is by constituting in the following high molecular polymer a kind of or two or more the mixing by any part by weight:
Urethane;
Polycarbonate;
SE;
Polymethylmethacrylate;
Phenoxy resin;
Polyester;
Ethylene copolymer;
In the above organic carrier, said polyester is polyethyleneterephthalate, polybutylene terephthalate, poly terephthalic acid diallyl, ekonol, unsaturated polyester resin, resol or vinyl resin;
In the above organic carrier; The polymkeric substance that said ethylene copolymer is formed by two or more monomer copolymerization that contains vinyl, the said monomer that contains vinyl has: vinyl acetate, vinyl alcohol, vinylchlorid, vinylidene chloride, vinylbenzene, vinyl cyanide, hydroxyalkyl acrylates, TEB 3K, methyl acrylate, ethyl propenoate, n-butyl acrylate and 2-ETHYL HEXYL ACRYLATE;
(3) organic solvent 8 ~ 72%
Said organic solvent is selected a kind of solvent in following ether solvent, esters solvent, ketones solvent and the alcoholic solvent, and perhaps two or more solvents are pressed the mixture of any part by weight:
Ether solvent has:
Diethylene glycol ether;
Propylene glycol monomethyl ether;
Dipropylene glycol methyl ether;
The dipropylene glycol propyl ether;
Propylene glycol propyl ether;
The Ucar 35 butyl ether;
The dipropylene glycol butyl ether;
The tripropylene glycol butyl ether;
The Ucar 35 phenylate;
The dipropylene glycol dme;
Esters solvent has:
ETHYLE ACETATE;
The diethylene glycol monobutyl ether acetic ester;
1-Methoxy-2-propyl acetate;
Dipropylene glycol methyl ether acetate;
PGDA;
The amyl acetate-n mixture;
N-butyl acetate;
Isobutyl acetate;
N-propyl acetate;
Iso Butyl Acetate;
N-butyl propionate;
The 3-ethoxyl ethyl propionate;
Witcizer 300;
The propionic acid n-pentyl ester;
The propionic acid n-propyl;
Dibasic acid esters;
Ketones solvent has:
Acetone;
Butanone;
Alcoholic solvent has:
α-or β-Terpineol 350;
Diethylene glycol monobutyl ether;
Hexylene glycol;
Amyl alcohol mixture;
Propyl carbinol;
Isopropylcarbinol;
Virahol;
Diisobutyl carbinol(DIBC);
Methyl isobutyl carbinol;
The 2-methyl butanol;
Pentyl alcohol;
N-propyl alcohol;
Exxal 12.
2. used for printed circuit catalytic ink according to claim 1 is characterized in that:
The content of said functional materials is 40 ~ 80%;
The content of said organic carrier is 3 ~ 15%;
The content of said organic solvent is 16 ~ 48%.
3. used for printed circuit catalytic ink according to claim 2 is characterized in that:
The content of said functional materials is 50 ~ 75%;
The content of said organic carrier is 5 ~ 10%;
The content of said organic solvent is 20 ~ 40%.
4. used for printed circuit catalytic ink according to claim 1; It is characterized in that: include auxiliary agent in the said catalytic ink; Said auxiliary agent has dispersion agent 0.2 ~ 1.5%; That dispersion agent adopts is cationic, a kind of in anionic, non-ionic type and the amphoteric, and wherein, cationic have polymine, the two ammonio methacrylates of two octadecyl or an imidazoline quaternary ammonium salt; Anionic is a soybean lecithin; Non-ionic type is an AEO; Amphoteric is the cocoyl azochlorosulfonate propyl lycine.
5. used for printed circuit catalytic ink according to claim 4 is characterized in that: said auxiliary agent has reductive agent 1 ~ 5%, and reductive agent adopts at least a in glucose, formaldehyde, inferior sodium phosphate, boranes material and the Hydrazine Hydrate 80.
6. according to claim 4 or 5 described used for printed circuit catalytic inks, it is characterized in that: said auxiliary agent has thixotropic agent 0.2 ~ 2%, and thixotropic agent adopts nano-carbon powder, nano silicon or organobentonite.
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| CN102827513A (en) * | 2012-09-04 | 2012-12-19 | 上海蓝沛新材料科技股份有限公司 | Photopolymerisable catalytic printing ink and application thereof |
| CN104376894A (en) * | 2014-11-26 | 2015-02-25 | 江苏欧耐尔新型材料有限公司 | Solar cell conductive positive silver pulp |
| CN105855535A (en) * | 2016-05-12 | 2016-08-17 | 苏州晶讯科技股份有限公司 | Method for preparing iron powder capable of being used for making seed ink |
| CN105925059A (en) * | 2016-05-12 | 2016-09-07 | 苏州晶讯科技股份有限公司 | Seed ink |
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| CN107636083A (en) * | 2015-05-27 | 2018-01-26 | 爱克发-格法特公司 | Metal nanoparticle dispersion |
| CN110045864A (en) * | 2019-03-06 | 2019-07-23 | 苏州蓝沛光电科技有限公司 | The preparation method of seed layer |
| CN110058726A (en) * | 2019-03-06 | 2019-07-26 | 苏州蓝沛光电科技有限公司 | The preparation method of touch screen |
| CN110058725A (en) * | 2019-03-06 | 2019-07-26 | 苏州蓝沛光电科技有限公司 | The preparation method of touch screen |
| CN111171685A (en) * | 2019-11-18 | 2020-05-19 | 深圳市荣伟业电子有限公司 | Tin surface protective agent special for manufacturing precise circuit board circuit and production method thereof |
| US11270809B2 (en) | 2017-03-16 | 2022-03-08 | Asahi Kasei Kabushiki Kaisha | Dispersing element, method for manufacturing structure with conductive pattern using the same, and structure with conductive pattern |
| US11328835B2 (en) | 2017-03-16 | 2022-05-10 | Asahi Kasei Kabushiki Kaisha | Dispersing element, method for manufacturing structure with conductive pattern using the same, and structure with conductive pattern |
| US11760895B2 (en) * | 2017-07-27 | 2023-09-19 | Asahi Kasei Kabushiki Kaisha | Copper oxide ink and method for producing conductive substrate using same, product containing coating film and method for producing product using same, method for producing product with conductive pattern, and product with conductive pattern |
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| CN102827513B (en) * | 2012-09-04 | 2015-04-22 | 上海蓝沛新材料科技股份有限公司 | Photopolymerisable catalytic printing ink and application thereof |
| CN102827513A (en) * | 2012-09-04 | 2012-12-19 | 上海蓝沛新材料科技股份有限公司 | Photopolymerisable catalytic printing ink and application thereof |
| CN104376894A (en) * | 2014-11-26 | 2015-02-25 | 江苏欧耐尔新型材料有限公司 | Solar cell conductive positive silver pulp |
| CN107636083A (en) * | 2015-05-27 | 2018-01-26 | 爱克发-格法特公司 | Metal nanoparticle dispersion |
| CN105855535A (en) * | 2016-05-12 | 2016-08-17 | 苏州晶讯科技股份有限公司 | Method for preparing iron powder capable of being used for making seed ink |
| CN105925059A (en) * | 2016-05-12 | 2016-09-07 | 苏州晶讯科技股份有限公司 | Seed ink |
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Application publication date: 20120718 |